CN109338283A - A kind of pack carburizing prepares the method and porous material of porous material - Google Patents
A kind of pack carburizing prepares the method and porous material of porous material Download PDFInfo
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- CN109338283A CN109338283A CN201811479111.XA CN201811479111A CN109338283A CN 109338283 A CN109338283 A CN 109338283A CN 201811479111 A CN201811479111 A CN 201811479111A CN 109338283 A CN109338283 A CN 109338283A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
- C23C8/64—Carburising
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
- C04B35/5618—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium aluminium carbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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Abstract
The present invention relates to the preparation methods of porous material, provide a kind of method that pack carburizing prepares porous material, comprising: are uniformly mixed titanium valve and aluminium powder and obtain mixed metal powder；Mixed metal powder pre-molding is obtained into green compact；Green compact are sintered under vacuum conditions, obtain Ti-Lu porous material；Ti-Lu porous material is placed in graphite boat, and fills alumina hollow ball and carbon black powder into graphite boat；After filling by graphite boat be placed in 800~1000 DEG C, vacuum degree be 6.0 × 10‑3Pa~1.6 × 10‑2It is sintered in the environment of Pa, sintering time is 8~10h.Porous material is made using the method that above-mentioned pack carburizing prepares porous material.The mechanical strength with higher of porous material made from the method provided through the invention and corrosion resistance.
Description
Technical field
The present invention relates to the preparation technical fields of porous material, prepare porous material in particular to a kind of pack carburizing
The method and porous material of material.
Background technique
TiAl intermetallic compound becomes Aeronautics and Astronautics neck with its low-density, good elevated temperature strength and antioxygenic property
The quite potential high-temperature structural material in domain.It is more to have had both metal because it is with metallic bond and covalent bond for TiAl intermetallic compound
The excellent high temperature resistant property of Porous materials and mechanical property, the acid-alkali-corrosive-resisting of ceramic porous material, but in practical application mistake
Cheng Zhong, antiacid caustic corrosion are still to be improved.
Ternary layered Ti2AlC is a kind of novel structural ceramic material, and good thermal conductivity, electric conductivity and room temperature are anti-
Destructiveness, excellent anti-thermal shock and high-temperature oxidation resistance, antiacid caustic corrosion, the easily characteristics such as processability, but its room temperature is drawn
It is low compared with TiAl intermetallic compound to stretch performance, limits its application.
In consideration of it, special propose the application.
Summary of the invention
The present invention provides a kind of methods that pack carburizing prepares porous material, it is intended to improve existing porous material and be difficult to
The problem of having both high mechanical strength corrosion resistance and good.
The present invention also provides a kind of porous material, mechanical strength with higher and preferable corrosion resistance.
The present invention is implemented as follows:
A kind of method that pack carburizing prepares porous material, comprising:
Titanium valve and aluminium powder are uniformly mixed and obtain mixed metal powder, the mass ratio of titanium valve and aluminium powder is 65~69:33；
Mixed metal powder pre-molding is obtained into green compact；
Green compact are sintered under vacuum conditions, are warming up to the heating rate less than 15 DEG C/min through the first stage
190~210 DEG C, keep the temperature 1.8~2.2h；Continue to be warming up to 600~640 through second stage with the heating rate less than 20 DEG C/min
DEG C, keep the temperature 2.8~3.3h；Continue to be warming up to 1280~1350 DEG C with the phase III of the heating rate less than 25 DEG C/min, protect
2~4h of temperature；It is cooled to room temperature to obtain Ti-Lu porous material through temperature-fall period with the rate of temperature fall less than 18 DEG C/min；
Ti-Lu porous material is placed in graphite boat, and fills alumina hollow ball and carbon black powder, oxygen into graphite boat
The mass ratio for changing aluminium hollow sphere and carbon black powder is 68~72:30；
After filling by graphite boat be placed in 800~1000 DEG C, vacuum degree be 6.0 × 10-3Pa~1.6 × 10-2The ring of Pa
It is sintered under border, sintering time is 8~10h.
A kind of porous material is made using the method that above-mentioned pack carburizing prepares porous material.
The beneficial effects of the present invention are: the pack carburizing that the present invention obtains by above-mentioned design prepares the side of porous material
Method, due to be made under the roasting condition of reasonable heating, heat preservation and cooling using properly mixed titanium valve and aluminium powder have compared with
Then Ti-Lu porous material is placed in by the Ti-Lu porous material of high mechanical strength together in alumina hollow ball and carbon black powder again
It is roasted 8~10 hours under conditions of suitable temperature suitable vacuum degree in graphite boat, so that porous material obtained is in hole
Ti is formed inside gap2AlC infiltration layer, and then porous material obtained has higher mechanical strength and excellent acidresistant property
Porous material.
The porous material that the present invention obtains by above-mentioned design, it is porous due to being prepared using pack carburizing provided by the invention
The method of material is made, therefore the porous material high mechanical strength, acidresistant property are good.
Detailed description of the invention
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention
Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as
It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the method that pack carburizing of the present invention prepares porous material, after filling boat, the structural schematic diagram in graphite boat；
Fig. 2 is the carburizing XRD diagram of porous material obtained.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
A kind of method that pack carburizing prepares porous material is provided to the embodiment of the present invention below to be specifically described.
A kind of method that pack carburizing prepares porous material, comprising:
S1, it titanium valve and aluminium powder is uniformly mixed obtains mixed metal powder, the mass ratio of titanium valve and aluminium powder is 65~69:
33。
Specifically, it stocks up first.Titanium valve and aluminium powder are weighed, so that the mass ratio of carbon dust and aluminium powder is 65~69:
33.Obtained titanium valve will be weighed and aluminium powder is uniformly mixed, it is preferable that in order to enable titanium valve and aluminium powder can be sufficiently mixed uniform obtain
Mill ball is added thereto to mixed metal powder by titanium valve, aluminium powder to be placed in ball mill, using mill ball as medium, mixing 8
~10h, it is preferable that the mass ratio of the additional amount of mill ball and mixed metal powder is 3~5:1, so that titanium valve, aluminium powder and drying
Active powdered carbon be uniformly mixed.
Further, to make porous material gap obtained be evenly distributed, the granularity of titanium valve is -200 mesh~+325 mesh,
The granularity of aluminium powder is -200 mesh~+325 mesh.- 200 mesh~+325 mesh, which refer to, can not pass through 325 meshes by 200 mesh screens
The particle size range of net.
S2, mixed metal powder pre-molding is obtained into green compact.
Mixed metal powder is placed in the mold of Φ 25mm, applies 190~220MPa pressure compression moulding to it and obtain cake
Shape green compact, the green compact of pie can be sintered to obtain the porous material of pie, more efficient convenient for subsequent carburizing process.
S3, green compact are sintered under vacuum conditions, are heated up with the heating rate less than 15 DEG C/min through the first stage
To 190~210 DEG C, 1.8~2.2h is kept the temperature；Continue to be warming up to 600 through second stage with the heating rate less than 20 DEG C/min~
640 DEG C, keep the temperature 2.8~3.3h；Continue to be warming up to 1280~1350 DEG C with the phase III of the heating rate less than 25 DEG C/min,
Keep the temperature 2~4h；It is cooled to room temperature to obtain Ti-Lu porous material through temperature-fall period with the rate of temperature fall less than 18 DEG C/min.
Specifically, green compact that S2 step obtains are sintered under vacuum conditions as being placed in vacuum sintering furnace, are passed through
First stage is warming up to 190~210 DEG C, keeps the temperature 1.8~2.2h, and the heating rate of first stage heating is less than 15 DEG C/min；
Then 600~640 DEG C are warming up to through second stage, keep the temperature 2.8~3.3h, second stage heating rate is less than 20 DEG C/min；
Then the phase III is warming up to 1280~1350 DEG C, keeps the temperature 2~4h, and phase III heating rate is less than 25 DEG C/min.Most
Ti-Lu porous material is obtained with rate of temperature fall cooling down to the room temperature less than 18 DEG C/min afterwards.
The porous material that green compact obtained are sintered under above-mentioned heating, heat preservation and cooling conditions under S2 step pressure,
Effectively green compact can be avoided to deform.
Preferably, for guarantee preparation efficiency it is enough high and further such that obtained Ti-Lu porous material apparent porosity
Height, the heating rate of first stage heating are 9~11 DEG C/min.
Preferably, for be further ensured that preparation efficiency and further such that obtained Ti-Lu porous material apparent porosity
Height, the heating rate of two sections of heatings are 14~16 DEG C/min.
Preferably, for be further ensured that preparation efficiency and further such that obtained Ti-Lu porous material apparent porosity
Height, the heating rate of phase III heating are 18~22 DEG C/min.
Preferably, for be further ensured that preparation efficiency and further such that obtained Ti-Lu porous material apparent porosity
Height, the rate of temperature fall of temperature-fall period are 10~15 DEG C/min.
S4, Ti-Lu porous material is placed in graphite boat, and fills alumina hollow ball and carbon black powder into graphite boat,
Alumina hollow ball and the mass ratio of carbon black powder are 68~72:30.
Ti-Lu porous material made from S3 is placed in graphite boat, and fills alumina hollow ball and carbon black into graphite boat
Powder, due to the Ti-Lu porous material being usually placed in graphite boat quantity be it is multiple, multiple Ti-Lu porous materials be in pie, filling out
When filling alumina hollow ball and carbon black powder, it can be covered after placing a Ti-Lu porous material to this Ti-Lu porous material surface
Lid alumina hollow ball and carbon black powder after covering is enough, then place next Ti-Lu porous material, then proceed to filling aluminium oxide
Hollow sphere and carbon black powder, are recycled with this, until filling up graphite boat, are covered tightly graphite boat lid after filling up graphite boat, are filled graphite boat after boat
Interior structural schematic diagram is as shown in Figure 1.Preferably, in order to enable carbon and alumina amount are reacted with Ti-Lu porous material enough, phase
The distance between adjacent Ti-Lu porous material is 1~2cm.
More specifically, graphite boat is 6~10cm of diameter, the cylindrical shape of high 5~8cm.
After S5, filling by graphite boat be placed in 800~1000 DEG C, vacuum degree be 6.0 × 10-3Pa~1.6 × 10-2Pa
In the environment of be sintered, sintering time be 8~10h.Sintering obtains porous material provided by the invention.
The method that pack carburizing provided by the invention prepares porous material is sintered between preparation TiAl metal using priming reaction
Compound porous material, and as matrix, Ti is formed in pore interior using pack carburizing method2AlC infiltration layer, so that being made
Porous material be able to maintain the mechanical strength and Ti of TiAl metal polyporous material2AlC excellent acidresistant property.
The present invention also provides the porous materials as made from the above method.
Prepared by the method for porous material and porous to a kind of pack carburizing provided by the invention below in conjunction with specific embodiment
Material is specifically described.
Embodiment 1
It present embodiments provides a kind of pack carburizing and prepares the method for porous material and the porous material as made from this method
Material.
A kind of method that pack carburizing prepares porous material, comprising: titanium valve 65g, aluminium powder 33g will be weighed, by titanium valve, aluminium powder
The mill ball for being put into 300g is placed in ball mill as medium, and mixing 8h is uniformly mixed and obtains mixed metal powder, selected titanium
The granularity of powder and aluminium powder is -200 mesh~+325 mesh.
Mixed metal powder is placed in the mold of Φ 25mm, applies 190MPa pressure compression moulding to it and obtain pie life
Base.
Green compact are placed under vacuum condition and are sintered, are warming up to 210 DEG C with the heating rate 11 DEG C/min first stage,
1.8h is kept the temperature, 640 DEG C is warming up to through second stage with 16 DEG C/min of heating rate, 2.8h is kept the temperature, with 22 DEG C/min of heating rate
Phase III is warming up to 1350 DEG C, is kept the temperature 2h, is then down to room temperature with the rate of temperature fall of 15 DEG C/min and obtains the porous material of titanium aluminium
Material.
Obtained pie Ti-Lu porous material is placed in diameter 6cm, in the cylinder-shaped graphite boat of high 5cm, and to graphite boat
The mass ratio of interior filling alumina hollow ball and carbon black powder, alumina hollow ball and carbon black powder is 68:30.Adjacent cake in graphite boat
Shape porous material is spaced about 1cm, after material installs in graphite boat, covers graphite boat lid.
By the graphite boat for having filled material be placed in 800 DEG C, vacuum degree be 6.0 × 10-3It is sintered in the environment of Pa, sintering time
For 10h.Porous material provided by the invention is obtained after sintering.
Embodiment 2
It present embodiments provides a kind of pack carburizing and prepares the method for porous material and the porous material as made from this method
Material.
A kind of method that pack carburizing prepares porous material, comprising: titanium valve 69g, aluminium powder 33g will be weighed, by titanium valve, aluminium powder
The mill ball for being put into 500g is placed in ball mill as medium, and mixing 10h is uniformly mixed and obtains mixed metal powder, selected
The granularity of titanium valve and aluminium powder is -200 mesh~+325 mesh.
Mixed metal powder is placed in the mold of Φ 25mm, applies 220MPa pressure compression moulding to it and obtain pie life
Base.
Green compact are placed under vacuum condition and are sintered, are warming up to 190 DEG C with the heating rate 9 DEG C/min first stage,
2.2h is kept the temperature, 600 DEG C is warming up to through second stage with 14 DEG C/min of heating rate, 3.3h is kept the temperature, with 18 DEG C/min of heating rate
Phase III is warming up to 1280 DEG C, is kept the temperature 4h, is then down to room temperature with the rate of temperature fall of 10 DEG C/min and obtains the porous material of titanium aluminium
Material.
Obtained pie Ti-Lu porous material is placed in diameter 10cm, in the cylinder-shaped graphite boat of high 8cm, and to graphite boat
The mass ratio of interior filling alumina hollow ball and carbon black powder, alumina hollow ball and carbon black powder is 72:30.Adjacent cake in graphite boat
Shape porous material is spaced about 2cm, after material installs in graphite boat, covers graphite boat lid.
By the graphite boat for having filled material be placed in 900 DEG C, vacuum degree be 1.6 × 10-2It is sintered in the environment of Pa, sintering time
For 8h.Porous material provided by the invention is obtained after sintering.
Embodiment 3
It present embodiments provides a kind of pack carburizing and prepares the method for porous material and the porous material as made from this method
Material.
A kind of method that pack carburizing prepares porous material, comprising: titanium valve 67g, aluminium powder 33g will be weighed, by titanium valve, aluminium powder
The mill ball for being put into 400g is placed in ball mill as medium, and mixing 9h is uniformly mixed and obtains mixed metal powder, selected titanium
The granularity of powder and aluminium powder is -200 mesh~+325 mesh.
Mixed metal powder is placed in the mold of Φ 25mm, applies 200MPa pressure compression moulding to it and obtain pie life
Base.
Green compact are placed under vacuum condition and are sintered, are warming up to 200 DEG C with the heating rate 10 DEG C/min first stage,
2h is kept the temperature, 620 DEG C is warming up to through second stage with 15 DEG C/min of heating rate, keeps the temperature 3h, with 20 DEG C/min of heating rate through the
Three step-up temperatures keep the temperature 3h, are then down to room temperature with the rate of temperature fall of 12 DEG C/min and obtain Ti-Lu porous material to 1300 DEG C.
Obtained pie Ti-Lu porous material is placed in diameter 8cm, in the cylinder-shaped graphite boat of high 6cm, and to graphite boat
The mass ratio of interior filling alumina hollow ball and carbon black powder, alumina hollow ball and carbon black powder is 70:30.Adjacent cake in graphite boat
Shape porous material is spaced about 1.5cm, after material installs in graphite boat, covers graphite boat lid.
By the graphite boat for having filled material be placed in 1000 DEG C, vacuum degree be 1.0 × 10-2It is sintered in the environment of Pa, when sintering
Between be 9h.Porous material provided by the invention is obtained after sintering.
Embodiment 4
It present embodiments provides a kind of pack carburizing and prepares the method for porous material and the porous material as made from this method
Material.
A kind of method that pack carburizing prepares porous material, comprising: titanium valve 66g, aluminium powder 33g will be weighed, by titanium valve, aluminium powder
The mill ball for being put into 300g is placed in ball mill as medium, and mixing 9h is uniformly mixed and obtains mixed metal powder, selected titanium
The granularity of powder and aluminium powder is -200 mesh~+325 mesh.
Mixed metal powder is placed in the mold of Φ 25mm, applies 210MPa pressure compression moulding to it and obtain pie life
Base.
Green compact are placed under vacuum condition and are sintered, are warming up to 200 DEG C with the heating rate 10 DEG C/min first stage,
2.1h is kept the temperature, 620 DEG C is warming up to through second stage with 15 DEG C/min of heating rate, 3.1h is kept the temperature, with 20 DEG C/min of heating rate
Phase III is warming up to 1300 DEG C, keeps the temperature 3.5h, and being then down to room temperature with the rate of temperature fall of 14 DEG C/min, to obtain titanium aluminium porous
Material.
Obtained pie Ti-Lu porous material is placed in diameter 9cm, in the cylinder-shaped graphite boat of high 7cm, and to graphite boat
The mass ratio of interior filling alumina hollow ball and carbon black powder, alumina hollow ball and carbon black powder is 71:30.Adjacent cake in graphite boat
Shape porous material is spaced about 1.2cm, after material installs in graphite boat, covers graphite boat lid.
By the graphite boat for having filled material be placed in 950 DEG C, vacuum degree be 1.2 × 10-2It is sintered in the environment of Pa, sintering time
For 9.5h.Porous material provided by the invention is obtained after sintering.
Embodiment 5
It present embodiments provides a kind of pack carburizing and prepares the method for porous material and the porous material as made from this method
Material.
A kind of method that pack carburizing prepares porous material, comprising: titanium valve 67g, aluminium powder 33g will be weighed, by titanium valve, aluminium powder
The mill ball for being put into 300g is placed in ball mill as medium, and mixing 9h is uniformly mixed and obtains mixed metal powder, selected titanium
The granularity of powder and aluminium powder is -200 mesh~+325 mesh.
Mixed metal powder is placed in the mold of Φ 25mm, applies 190MPa pressure compression moulding to it and obtain pie life
Base.
Green compact are placed under vacuum condition and are sintered, are warming up to 200 DEG C with the heating rate 10 DEG C/min first stage,
1.9h is kept the temperature, 630 DEG C is warming up to through second stage with 15 DEG C/min of heating rate, 2.9h is kept the temperature, with 20 DEG C/min of heating rate
Phase III is warming up to 1330 DEG C, keeps the temperature 2.5h, and being then down to room temperature with the rate of temperature fall of 14 DEG C/min, to obtain titanium aluminium porous
Material.
Obtained pie Ti-Lu porous material is placed in diameter 8cm, in the cylinder-shaped graphite boat of high 5cm, and to graphite boat
The mass ratio of interior filling alumina hollow ball and carbon black powder, alumina hollow ball and carbon black powder is 70:30.Adjacent cake in graphite boat
Shape porous material is spaced about 1.4cm, after material installs in graphite boat, covers graphite boat lid.
By the graphite boat for having filled material be placed in 950 DEG C, vacuum degree be 8 × 10-3It is sintered in the environment of Pa, sintering time is
8.5h.Porous material provided by the invention is obtained after sintering.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, the difference is that, the heating of the first stage heating of first sintering
Rate is 14 DEG C/min.
Embodiment 7
The present embodiment is substantially the same manner as Example 3, the difference is that, the heating of the second stage heating of first sintering
Rate is 18 DEG C/min.
Embodiment 8
The present embodiment is substantially the same manner as Example 3, the difference is that, the heating of the phase III heating of first sintering
Rate is 24 DEG C/min.
Embodiment 9
The present embodiment is substantially the same manner as Example 3, the difference is that, the rate of temperature fall of the temperature-fall period of first sintering
For 17 DEG C/min.
Comparative example 1
This comparative example is substantially the same manner as Example 3, the difference is that, the heating in the first heating stage of first sintering
Rate is 20 DEG C/min.
Comparative example 2
This comparative example is substantially the same manner as Example 3, the difference is that, the heating of the second stage heating of first sintering
Rate is 25 DEG C/min.
Comparative example 3
This comparative example is substantially the same manner as Example 3, the difference is that, the heating of the phase III heating of first sintering
Rate is 30 DEG C/min.
Comparative example 4
This comparative example is substantially the same manner as Example 3, the difference is that, the rate of temperature fall of the temperature-fall period of first sintering
For 21 DEG C/min.
Comparative example 5
This comparative example is substantially the same manner as Example 3, the difference is that, being placed in the temperature being sintered in graphite boat for the second time is
700℃。
Comparative example 6
This comparative example is substantially the same manner as Example 3, the difference is that, being placed in the temperature being sintered in graphite boat for the second time is
1200℃。
Comparative example 7
This comparative example is substantially the same manner as Example 3, the difference is that, it is placed in sintering 6 hours in graphite boat for the second time.
Comparative example 8
This comparative example is substantially the same manner as Example 3, the difference is that, it is placed in sintering 12 hours in graphite boat for the second time.
Experimental example 1
By Ti-Lu porous material obtained in embodiment 3 and embodiment 6-9 preparation process and finally obtained porous material
Material is soaked in the sulfuric acid solution of hydrochloric acid and 0.5mol/L that concentration is 0.5mol/L respectively, detects its corrosive nature, will be weightless
Rate is recorded to table 1.The final porous material obtained of embodiment 3 is subjected to X and is accused of diffraction, X-ray diffractogram is as shown in Figure 2.
The weight-loss ratio (%) of porous material corrosion experiment obtained in each embodiment preparation process of table 1
, it can be seen that embodiment 3 is during preparing porous material from table 1, Ti-Lu porous material obtained and
The corrosion resistance of final porous material obtained is better than embodiment 6-9.Illustrate liter of present invention during first sintering
The good corrosion resistance of porous material obtained when warm rate and rate of temperature fall are in this preferred scope.
Porosity through detection embodiment 3 Ti-Lu porous material obtained during preparing porous material is 46%,
15.6 μm of average pore size, thus, it is possible to illustrate, during the present invention prepares porous material, intermediate product titanium aluminium obtained is porous
The porosity of material is high.
Fig. 2 can be seen that in TiAl and Ti3Al2On the basis of object phase, there is stronger Ti2The peak AlC illustrates that TiAl is porous
Material surface has obtained Ti2The carburized layer of AlC.
Experimental example 2
Ti-Lu porous material obtained in 3 porous material preparation process of embodiment and embodiment 3 is final obtained more
Finally porous material obtained is soaked in hydrochloric acid that concentration is 0.5mol/L and 0.5mol/L respectively by Porous materials and comparative example 1-8
In sulfuric acid solution, its corrosive nature is detected, weight-loss ratio is recorded to table 2.
The weight-loss ratio (%) of each embodiment of table 2 and comparative example corrosion experiment
By table 2, it can be seen that weight-loss ratio is apparently higher than embodiment 3 after each comparative example 30 days, and by each comparative example of table 2
It is compared with each embodiment of table 1, it will be obvious that, each embodiment corrosion resistance of the invention is above comparative example.
It can be seen that in the preparation process of porous material, the heating efficiency and drop of each temperature rise period baked for the first time
The cooling efficiency of thermophase the present invention claims in the range of when, the corrosive nature of porous material obtained can be significantly improved.
And bake for the second time bake temperature and bake the time the present invention claims in the range of when, the corrosion of porous material obtained
Performance is more preferable.
Experimental example 3
By Ti-Lu porous material obtained in embodiment 1 to 9 preparation process of embodiment and final obtained porous material into
Row stretching experiment measures the tensile strength of each group material, record to table 3.
The tensile strength (MPa) of 3 each group material of table
By table 3, it can be seen that the tensile strength for the porous material that each group embodiment provides is higher, TiAl porous material
Tensile strength with higher itself, tensile strength is about 44~48.5MPa, and carburizing post-tensioning intensity is held essentially constant.
In conclusion porous material provided by the invention, due to using properly mixed titanium valve and aluminium powder reasonable heating,
The Ti-Lu porous material with higher mechanical strength is made under the roasting condition of heat preservation and cooling, then again by the porous material of titanium aluminium
Expect to be placed in together in graphite boat in alumina hollow ball and carbon black powder and be roasted under conditions of suitable temperature suitable vacuum degree
It burns 8~10 hours, so that porous material obtained forms Ti in pore interior2AlC, and porous material obtained is being kept
Porous material with excellent acidresistant property while with higher mechanical strength.
Porous material provided by the invention, the method system due to preparing porous material using pack carburizing provided by the invention
, therefore the porous material high mechanical strength, acidresistant property are good.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method that pack carburizing prepares porous material characterized by comprising
Titanium valve and aluminium powder are uniformly mixed and obtain mixed metal powder, the mass ratio of titanium valve and aluminium powder is 65~69:33；
The mixed metal powder pre-molding is obtained into green compact；
The green compact are sintered under vacuum conditions, are warming up to the heating rate less than 15 DEG C/min through the first stage
190~210 DEG C, keep the temperature 1.8~2.2h；Continue to be warming up to 600~640 through second stage with the heating rate less than 20 DEG C/min
DEG C, keep the temperature 2.8~3.3h；Continue to be warming up to 1280~1350 DEG C with the phase III of the heating rate less than 25 DEG C/min, protect
2~4h of temperature；It is cooled to room temperature to obtain Ti-Lu porous material through temperature-fall period with the rate of temperature fall less than 18 DEG C/min；
The Ti-Lu porous material is placed in graphite boat, and fills alumina hollow ball and carbon black into the graphite boat
The mass ratio of powder, alumina hollow ball and carbon black powder is 68~72:30；
After filling by graphite boat be placed in 800~1000 DEG C, vacuum degree be 6.0 × 10-3Pa~1.6 × 10-2In the environment of Pa
Sintering, sintering time are 8~10h.
2. the method that pack carburizing according to claim 1 prepares porous material, which is characterized in that the titanium valve and described
Aluminium powder is uniformly mixed, and is to mix the titanium valve and the aluminium powder with mill ball, using the mill ball as 8~10h of medium mixing.
3. the method that pack carburizing according to claim 2 prepares porous material, which is characterized in that the mill ball adds
The mass ratio for entering amount and the mixed metal powder is 3~5:1.
4. the method that pack carburizing according to claim 1 prepares porous material, which is characterized in that the granularity of the titanium valve
For -200 mesh~+325 mesh, the granularity of the aluminium powder is -200 mesh~+325 mesh.
5. the method that pack carburizing according to claim 1 prepares porous material, which is characterized in that by the mixed metal
It is that the mixed metal powder is first fitted into application 190~220MPa pressure compression moulding in mold that powder pre-molding, which obtains green compact,；
Preferably, mould specification is Φ 25mm.
6. the method that pack carburizing according to claim 1 prepares porous material, which is characterized in that be placed in graphite boat
The Ti-Lu porous material quantity be it is multiple, at a distance of 1~2cm between upper and lower two Ti-Lu porous materials, and adjacent
Alumina hollow ball and carbon black powder are full of between the Ti-Lu porous material.
7. the method that pack carburizing according to claim 6 prepares porous material, which is characterized in that the porous material of titanium aluminium
Material is in pie.
8. the method that pack carburizing according to claim 6 prepares porous material, which is characterized in that the graphite boat is straight
6~10cm of diameter, the cylindrical shape of high 5~8cm.
9. the method that pack carburizing according to claim 1 prepares porous material, which is characterized in that the first stage liter
The heating rate of temperature is 9~11 DEG C/min；
Preferably, the heating rate of the second stage heating is 14~16 DEG C/min；
Preferably, the heating rate of the phase III heating is 18~22 DEG C/min；
Preferably, the rate of temperature fall of the temperature-fall period is 10~15 DEG C/min.
10. a kind of porous material, which is characterized in that prepare porous material using the pack carburizing such as any one of claim 1-9
Method be made.
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